CN109174200A - A kind of catalyst, preparation method and synthetic method synthesizing 1,1- diethoxyethane - Google Patents
A kind of catalyst, preparation method and synthetic method synthesizing 1,1- diethoxyethane Download PDFInfo
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- CN109174200A CN109174200A CN201811042927.6A CN201811042927A CN109174200A CN 109174200 A CN109174200 A CN 109174200A CN 201811042927 A CN201811042927 A CN 201811042927A CN 109174200 A CN109174200 A CN 109174200A
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- diethoxyethane
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- metal halide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/28—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of the platinum group metals, iron group metals or copper
- B01J31/30—Halides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/28—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of the platinum group metals, iron group metals or copper
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/32—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of manganese, technetium or rhenium
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/48—Preparation of compounds having groups
- C07C41/50—Preparation of compounds having groups by reactions producing groups
Abstract
The invention discloses a kind of catalyst for synthesizing 1,1- diethoxyethane, including metal halide and the molar ratio containing nitrogen complex, the metal halide and containing nitrogen complex are 1:0.5-8.Above-mentioned catalyst is added in dehydrated alcohol, the dehydrated alcohol is placed under oxygen atmosphere, purity oxygen or oxygenous mixed gas are passed through into the dehydrated alcohol, in 100 DEG C -140 DEG C, it is reacted under speed of agitator 300-800r/min, 1,1- diethoxyethane is made.Catalyst of the invention includes containing nitrogen complex and metal halide, has the advantages that catalytic activity is high, and reaction speed is fast, and selectivity is high；And catalyst system small toxicity meets demand of the existing Production trend to green production.Metal halide in the catalyst accelerates the progress of oxidative addition, and the acid-base property of reaction system can be suitably adjusted simultaneously, carry out reaction to the direction for generating 1,1- diethoxyethane, mild reaction process also can be relieved corrosion of the reaction material liquid to stainless steel reaction equipment.
Description
Technical field
The invention belongs to technical field of chemical synthesis, and in particular to the synthetic method of one kind 1,1- diethoxyethane is somebody's turn to do
The preparation method of the catalyst being related in synthetic method and the catalyst.
Background technique
1,1- diethoxyethane (1,1-diethoxyethane) is one of ethyl alcohol major downstream product, has poison
The advantages that property is small, dissolubility is good, low boiling point；It is the synthesizing carbonyl compound such as important intermediate of ketone, aldehyde compound.1,1- simultaneously
Diethoxyethane is good with diesel oil intersolubility, and has excellent combustibility, biomass of the alternative ethyl alcohol as diesel oil
Particle and NO can be greatly reduced in oxygen-containing adding ingredientxDischarge, improve Cetane number, be that potential high-grade fuel and fuel add
Add agent.In addition to this, 1,1- diethoxyethane or a kind of novel high-grade fragrance and important synthetic intermediate, are widely used in
The industry of the additives such as cosmetics, food and organic synthesis.
The primary synthetic methods of 1,1- diethoxyethane have ethyl alcohol and acetaldehyde condensation reaction method, direct oxidation of ethylene to method,
Ethyl alcohol direct oxidation method etc..Currently, the production method of industrial comparative maturity is ethyl alcohol and acetaldehyde condensation reaction method, but the technique
There are process complexity, equipment seriously corroded, directly using toxic and the problems such as be difficult to the acetaldehyde saved for a long time.Therefore, in order to keep away
Exempt from directly to use acetaldehyde as raw material and improve the efficiency of 1,1- diethoxyethane synthesis, exploitation generates partial oxidation of ethanol
The catalysts selective of 1,1- diethoxyethane has become a hot research topic in recent years.
The TaO loaded respectively with silica5And Nb2O5Photochemical catalyst catalysis ethanol direct oxidation synthesizes 1,1- diethoxy
Base ethane, reaction generate a large amount of by-product, such as acetaldehyde, acetic acid and ethylene under aerobic conditions, are only to ethanol conversion
6.9%.
The RuO being carried on silica and tin oxide2, catalysis methanol and ethanol gas phase selectivity oxygen at 300-400K
It is melted into acetal, wherein RuO2/SnO2Catalyst obtains 81% 1,1- diethoxyethane selectivity and 15% at 393K
Low ethanol conversion ratio.Mo is used at 497K12V3W1.2Cu1.2Sb0.5OxCatalysis ethanol gas phase selective oxidation reaction, 1,1- bis-
The yield of Ethoxyethane is 14%.
And using alcohol as raw material, 1,1- diethoxyethane (acetal) is prepared by one step of method of selective oxidation, but remove
Outside dimethoxym ethane, other acetals are since thermodynamics limitation is difficult to obtain high yield, and the process is needed using a large amount of acid catalysts,
Environment is caused seriously to pollute.
Summary of the invention
It is an object of the present invention to: above-mentioned deficiency in the prior art is solved, an a kind of step oxidative synthesis 1 is provided,
The catalyst of 1- diethoxyethane, the catalyst effective active is high, easily recycles, advantages of environment protection, the catalyst
Ethyl alcohol liquid phase, one-step synthesis 1,1- diethoxyethane.
To achieve the goals above, the technical solution adopted by the present invention are as follows: a kind of synthesis 1,1- diethoxyethane is urged
Agent, including metal halide and the molar ratio containing nitrogen complex, the metal halide and containing nitrogen complex are 1:0.5-8.
The nitrogen complex that contains is 1,2- cyclohexanedionedioxime, dimethylglyoxime, glyoxime, the even acyl dioxime of α-sugar, benzil
Dioxime, 2,6- dichloro benzaldoxime, 1,4- benzoquinones dioxime, 5,7-dichloro-8-hydroxyquinoline, 10- hydroxy benzo [h] quinoline, 2,
5- diphenyl-1,3,4- diazole, 1- methyl-1-H pyrazoles, methylimidazole, benzimidazole, 2 hydroxy pyrimidine, 4,4'- diformazan
One of base -2,2'- bipyridyl, 2-aminopyridine are a variety of.
The metal halide is ruthenic chloride, stannous chloride, copper chloride, palladium chloride, manganese chloride, cobalt chloride, palladium bromide, bromine
Change one of copper, manganous bromide, ferric bromide, nickelous bromide or a variety of.Preferably, the metal halide is ruthenic chloride.Preferably
Metal halide is ruthenic chloride, Ru3+It is changed into the oxidisability of acetaldehyde and acetic acid with catalysis ethanol, is changed into Ru after reaction2+,
Ru2+Then in O2Under the action of be oxidized to Ru3+, this allows for ethyl alcohol while the oxidation reaction of completion, and catalyst also completes
Oxygen cycle, therefore RuCl3Can efficient catalysis ethanol oxidation reaction, it is reusable repeatedly；And RuCl3It is a kind of again
Mild lewis acid can make the acetaldehyde generated react condensation with feed ethanol and generate 1,1- diethoxyethane, therefore this is urged
Agent is again to 1,1- diethoxyethane selectivity with higher.
It is an object of the present invention to: a kind of method for preparing above-mentioned catalyst is provided, the preparation method is simple, high
It imitates, without the consersion unit of profession.
The technical solution of the present invention is as follows: including that the metal halide and the nitrogen complex that contains are massaged your 1:0.5-8
It is uniformly mixed.
The third object of the present invention is, provides a kind of one-step synthesis method 1, the method for 1- diethoxyethane, the synthesis
1, the 1- diethoxyethane selectivity of method is high, and the conversion ratio of ethyl alcohol is also higher, the materials safety used described in synthesis
It is nontoxic, it is small to the corrosivity of consersion unit.
Technical solution provided by the invention are as follows: above-mentioned catalyst is added in dehydrated alcohol, the dehydrated alcohol is set
Under oxygen atmosphere, purity oxygen or oxygenous mixed gas are passed through into the dehydrated alcohol, in 100 DEG C -140 DEG C, stirring
It is reacted under revolving speed 300-800r/min, 1,1- diethoxyethane is made.
Further, the air pressure of the purity oxygen is 1-3.5Mpa, in the oxygenous mixed gas, the partial pressure of oxygen
For 1-3.5Mpa.
Further, the oxygenous mixed gas includes component A and component B, and the component A is oxygen, and described group
Part B is one of nitrogen, argon gas, helium or a variety of, and the mass fraction of the component A is greater than 20% less than 100%.
Further, the mass ratio of the catalyst and the dehydrated alcohol is 1-20:4000.
By adopting the above-described technical solution, the beneficial effects of the present invention are:
Catalyst of the invention includes containing nitrogen complex and metal halide, has catalytic activity high, and reaction speed is fast, choosing
The advantages that selecting property is high；And catalyst system small toxicity meets demand of the existing Production trend to green production.In the catalyst
Metal halide accelerate the progress of oxidative addition, and can suitably adjust the acid-base property of reaction system simultaneously, make reaction to
The direction for generating 1,1- diethoxyethane carries out, and mild reaction process also can be relieved reaction material liquid to stainless steel reaction equipment
Corrosion.The preparation method of the catalyst is simple, is directly uniformly mixed two kinds of materials, is not necessarily to consersion unit.And no
It needs to pre-process catalyst, saves and the pretreated time is carried out to catalyst, while having ensured that catalyst system is urged
Change the stability of performance.
The method that 1,1- diethoxyethane is synthesized in the present invention contains nitrogen complex and metal halide with selectively high
As catalyst, oxygen is passed into ethyl alcohol liquid phase, reaction condition is mild, and the selectivity of 1,1- diethoxyethane is high, second
The by-product of the high conversion efficiency of alcohol, the synthetic method is few.
Specific embodiment
All features disclosed in this specification can group in any way other than mutually exclusive and/or step
It closes.All raw materials are commercially available in embodiment.
Comparative example 1:
39.5g ethyl alcohol is added into 250ml reaction kettle, is set at room temperature with oxygen 0.01g ruthenic chloride is added
The air to swap out in reaction kettle, then at 120 DEG C, it is the pure of 2MPa that air pressure is continually fed into the dehydrated alcohol into reaction kettle
Oxygen, under the stirring condition of 600r/min, cooling after reacting 3h, liquid product uses gas chromatographic analysis, calculates gained second
Alcohol conversion is 38.1%, and 1,1- diethoxyethane is selectively 78.0%.
Embodiment 1:
39.5g dehydrated alcohol is added into 250ml reaction kettle, then by 0.007g1,2- cyclohexanedionedioxime and 0.01g chlorine
The mixture for changing ruthenium is added in reaction kettle, at room temperature, goes out the air in reaction kettle with replacement of oxygen, then 120
At DEG C, the purity oxygen that air pressure is 2MPa is continually fed into the dehydrated alcohol into reaction kettle, under the stirring condition of 600r/min,
Cooling after reacting 3h, liquid product uses gas chromatographic analysis, calculate ethanol conversion is 32.7%, 1,1- diethoxy
Ethane is selectively 80.4%.
Embodiment 2:
It is added 39.5g dehydrated alcohol into 250ml reaction kettle, then by the mixed of 0.006g dimethylglyoxime and 0.01g ruthenic chloride
It closes object to be added in reaction kettle, at room temperature, goes out the air in reaction kettle with replacement of oxygen, then at 100 DEG C, to anti-
The purity oxygen for being continually fed into that air pressure is 1MPa in the dehydrated alcohol in kettle is answered, under the stirring condition of 800r/min, after reacting 3h,
Cooling, liquid product uses gas chromatographic analysis, ethanol conversion 25.3%, 1, and 1- diethoxyethane is selectively
87.0%.
Embodiment 3
39.5g dehydrated alcohol is added into 250ml reaction kettle, then by the mixing of 0.004g glyoxime and 0.01g ruthenic chloride
Object is added in reaction kettle, at room temperature, goes out the air in reaction kettle with replacement of oxygen, then at 130 DEG C, to reaction
The mixed gas of nitrogen and oxygen is continually fed into dehydrated alcohol in kettle, the partial pressure of oxygen is 2MPa in the mixed gas,
Under the stirring condition of 300r/min, cooling after reacting 4h, liquid product uses gas chromatographic analysis, and ethanol conversion is
30.4%, 1,1- diethoxyethane is selectively 82.1%.
Embodiment 4
39.5g dehydrated alcohol is added into 250ml reaction kettle, then by 0.009g2,6- dichloro benzaldoxime and 0.01g chlorine
The mixture for changing copper is added in reaction kettle, at room temperature, goes out the air in reaction kettle with replacement of oxygen, then 140
At DEG C, the mixed gas of argon gas and oxygen is continually fed into the dehydrated alcohol into reaction kettle, the mass fraction of oxygen is 80%,
The partial pressure of oxygen is 1MPa in the mixed gas, cooling after reacting 4.5h under the stirring condition of 400r/min, liquid product
Using gas chromatographic analysis, ethanol conversion 26.8%, 1,1- diethoxyethane is selectively 85.2%.
Embodiment 5
39.5g dehydrated alcohol is added into 250ml reaction kettle, then by 0.012g benzil dioxime and 0.01g chlorine cobalt chloride
Mixture be added in reaction kettle, at room temperature, go out the air in reaction kettle with replacement of oxygen, then at 140 DEG C,
The purity oxygen that air pressure is 3.5MPa is continually fed into dehydrated alcohol into reaction kettle, under the stirring condition of 300r/min, instead
Cooling after answering 3.5h, liquid product uses gas chromatographic analysis, ethanol conversion 25.9%, 1, the choosing of 1- diethoxyethane
Selecting property is 86.7%.
Embodiment 6
39.5g dehydrated alcohol is added into 250ml reaction kettle, then by 0.010g α-furil-dioxime and 0.01g palladium bromide
Mixture is added in reaction kettle, at room temperature, goes out the air in reaction kettle with replacement of oxygen, then at 130 DEG C, to
The mixed gas of nitrogen and oxygen is continually fed into dehydrated alcohol in reaction kettle, the mass fraction of oxygen is 30%, the mixing
The partial pressure of oxygen is 3.5MPa in gas, and under the stirring condition of 300r/min, cooling after reacting 3h, liquid product uses gas
Analysis of hplc, ethanol conversion 30.4%, 1,1- diethoxyethane are selectively 85.7%.
Embodiment 7
39.5g dehydrated alcohol is added into 250ml reaction kettle, then by 0.007g1,4- benzoquinones dioxime and 0.01g copper bromide
Mixture be added in reaction kettle, at room temperature, go out the air in reaction kettle with replacement of oxygen, then at 110 DEG C,
The purity oxygen that air pressure is 1MPa, under the stirring condition of 800r/min, reaction are continually fed into dehydrated alcohol into reaction kettle
Cooling after 4h, liquid product uses gas chromatographic analysis, ethanol conversion 29.7%, 1,1- diethoxyethane selectivity
It is 84.6%.
Embodiment 8
39.5g dehydrated alcohol is added into 250ml reaction kettle, then by 0.010g5,7- dichloro-8-hydroxyquinoline and 0.01g
The mixture of manganous bromide is added in reaction kettle, and other conditions are identical as comparative experiments example, and after reaction, ethanol conversion is
36.7%, 1,1- diethoxyethane is selectively 81.1%.
Embodiment 9
The mixture of 0.010g10- hydroxy benzo [h] quinoline and 0.01g ferric bromide is added in 39.5g ethyl alcohol, other
Condition is same as Example 1, and after reaction, ethanol conversion 32.9%, 1,1- diethoxyethane is selectively 84.7%.
Embodiment 10
By 0.010g2, the mixture of 5- diphenyl -1,3,4- diazole and 0.01g nickelous bromide is added in 39.5g ethyl alcohol,
Other conditions are same as Example 2, and after reaction, ethanol conversion 40.6%, 1,1- diethoxyethane is selectively
81.1%.
Embodiment 11
The mixture of 0.015g1- methyl-1-H pyrazoles and 0.01g cobalt chloride is added in 39.5g ethyl alcohol, other conditions
Same as Example 3, after reaction, ethanol conversion 36.1%, 1,1- diethoxyethane is selectively 85.9%.
Embodiment 12
The mixture of 0.005g methylimidazole and 0.01g copper bromide is added in 39.5g ethyl alcohol, other conditions and reality
It is identical to apply example 4, after reaction, ethanol conversion 37.0%, 1,1- diethoxyethane is selectively 87.8%.
Embodiment 13
The mixture of 0.006g benzimidazole and 0.01g manganous bromide is added in 39.5g ethyl alcohol, other conditions and implementation
Example 4 is identical, and after reaction, ethanol conversion 33.0%, 1,1- diethoxyethane is selectively 85.5%.
Embodiment 14
The mixture of 0.005g2- pyridone and 0.01g ruthenic chloride is added in 39.5g ethyl alcohol, other conditions and reality
It is identical to apply example 5, after reaction, ethanol conversion 32.4%, 1,1- diethoxyethane is selectively 81.9%.
Embodiment 15
The mixture of 0.009g4,4'- dimethyl -2,2'- bipyridyl and 0.01g nickelous bromide is added to 39.5g ethyl alcohol
In, other conditions are same as Example 6, and after reaction, ethanol conversion 31.5%, 1,1- diethoxyethane is selectively
80.7%.
Embodiment 16
The mixture of 0.005g2- aminopyridine and 0.01g copper chloride is added in 39.5g ethyl alcohol, other conditions and reality
It is identical to apply example 7, after reaction, ethanol conversion 30.8%, 1,1- diethoxyethane is selectively 86.0%.
Embodiment 17
Reaction condition is same as Example 2, the difference is that, in the present embodiment, 2,5- diphenyl -1,3,4- diazole
When being respectively 0.5:1,2:1,3:1 with the ratio between the amount of ruthenic chloride substance, after reaction ethanol conversion be respectively 38.7%,
41.1%, 39.0%, 1,1- diethoxyethane is selectively 83.8%, 84.9%, 85.2%.
Embodiment 18
When the catalyst system concentration is respectively 0.1g/L, 0.2g/L, 1g/L, 1,2- cyclohexanedionedioxime and ruthenic chloride object
When the ratio between amount of matter is 2:1, other conditions and implementation are 1 identical, after reaction ethanol conversion be respectively 31.7%, 41.1%,
42.8%, 1,1- diethoxyethane is selectively 86.7%, 84.9%, 75.2%.
Embodiment 19
When reaction temperature is respectively 100 DEG C, 120 DEG C, 140 DEG C, by 0.02g2,5- diphenyl -1,3,4- diazole and
0.01g ruthenic chloride is mixed to join in 39.5g ethyl alcohol, and other conditions are with comparative example 1, and ethanol conversion is respectively after reaction
26.8%, 41.1%, 45.1%, 1,1- diethoxyethane is selectively 87.9%, 84.9%, 57.5%.
Embodiment 20
When reaction pressure is respectively 1.0MPa, 2.0MPa, 3.5MPa, by 0.02g2,5- diphenyl -1,3,4- diazole and
0.01g ruthenic chloride is mixed to join in 39.5g ethyl alcohol, and other conditions are with comparative example 1, and ethanol conversion is respectively after reaction
29.4%, 41.1%, 43.2%, 1,1- diethoxyethane is selectively 83.2%, 84.9%, 67.7%.
Embodiment 21
When between being when reacted respectively 2h, 3h, 4.5h, by 0.02g2,5- diphenyl -1,3,4- diazole and 0.01g chlorination
Ruthenium is mixed to join in 39.5g ethyl alcohol, other conditions with comparative example 1, after reaction ethanol conversion be respectively 24.3%,
41.1%, 42.2%, 1,1- diethoxyethane is selectively 85.8%, 84.9%, 74.8%.
Embodiment 22
When speed of agitator is respectively 300r/min, 600r/min, 800r/min, by 0.02g2,5- diphenyl -1,3,4-
Diazole and 0.01g ruthenic chloride are mixed to join in 39.5g ethyl alcohol, and other conditions are with comparative example 1, and ethanol conversion is distinguished after reaction
It is 30.7%, 41.1%, 38.6%, 1,1- diethoxyethane is selectively 78.8%, 84.9%, 70.2%.
The high catalytic efficiency of catalyst of the invention it can be seen from the analysis result of above-described embodiment 1-22 utilizes this
The catalyst one-step synthesis method 1 of invention, 1- diethoxyethane, reaction step is simple, and the conversion ratio of ethyl alcohol can reach
45%, 1,1- diethoxyethane selectively can reach 87.9%.
The above, only highly preferred embodiment of the present invention, not to limit invention, scope of patent protection of the invention
It is subject to claims, it is all to change with equivalent processes made by specification of the invention and embodiment content, similarly
It should be included within the scope of the present invention.
Claims (9)
1. a kind of catalyst for synthesizing 1,1- diethoxyethane, it is characterised in that: including metal halide and contain nitrogen complex,
The metal halide and the molar ratio containing nitrogen complex are 1:0.5-8.
2. the catalyst of synthesis 1,1- diethoxyethane according to claim 1, it is characterised in that: the nitrogenous cooperation
Object is 1,2- cyclohexanedionedioxime, dimethylglyoxime, glyoxime, the even acyl dioxime of α-sugar, benzil dioxime, 2,6- dichlorobenzaldehyde
Oxime, 1,4- benzoquinones dioxime, 5,7-dichloro-8-hydroxyquinoline, 10- hydroxy benzo [h] quinoline, 2,5- diphenyl -1,3,4- diazole,
1- methyl-1-H pyrazoles, methylimidazole, benzimidazole, 2 hydroxy pyrimidine, 4,4'- dimethyl-2,2'- bipyridyl, 2- amino
One of pyridine is a variety of.
3. the catalyst of synthesis 1,1- diethoxyethane according to claim 1, it is characterised in that: the metal halide
Object be ruthenic chloride, stannous chloride, copper chloride, palladium chloride, manganese chloride, cobalt chloride, palladium bromide, copper bromide, manganous bromide, ferric bromide,
One of nickelous bromide is a variety of.
4. the catalyst of synthesis 1,1- diethoxyethane according to claim 3, it is characterised in that: the metal halide
Object is ruthenic chloride.
5. a kind of method for preparing catalyst according to any one of claims 1-4, it is characterised in that: including by the metal
Halide and it is described containing nitrogen complex in molar ratio 1:0.5-8 be uniformly mixed.
6. one kind 1, the synthetic method of 1- diethoxyethane, it is characterised in that: including by any catalysis of claim 1-4
Agent is added to absolute ethanol, and the dehydrated alcohol is placed under oxygen atmosphere, and purity oxygen is passed through into the dehydrated alcohol or is contained
The mixed gas of oxygen is reacted under 100 DEG C -140 DEG C, speed of agitator 300-800r/min.
7. the synthetic method of 1,1- diethoxyethane according to claim 6, it is characterised in that: the gas of the purity oxygen
Pressing is 1-3.5Mpa, and in the oxygenous mixed gas, the partial pressure of oxygen is 1-3.5Mpa.
8. the synthetic method of 1,1- diethoxyethane according to claim 7, it is characterised in that: described oxygenous mixes
Conjunction gas includes component A and component B, the component A are oxygen, and the component B is one of nitrogen, argon gas, helium or more
Kind, the mass fraction of the component A is greater than 20% less than 100%.
9. the synthetic method of 1,1- diethoxyethane according to claim 6, it is characterised in that: the catalyst and institute
The mass ratio for stating dehydrated alcohol is 1-20:4000.
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Citations (4)
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|---|---|---|---|---|
| CN102056880A (en) * | 2008-06-03 | 2011-05-11 | 阿克马法国公司 | Method for the synthesis of dialkoxy alkanes by means of the selective oxidation of alcohols |
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| DE102013220761A1 (en) * | 2013-10-15 | 2015-04-16 | Robert Bosch Gmbh | Precursor material and method for coating a substrate with a metal chalcogenide layer |
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2018
- 2018-09-04 CN CN201811042927.6A patent/CN109174200A/en active Pending
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|---|---|---|---|---|
| CN102056880A (en) * | 2008-06-03 | 2011-05-11 | 阿克马法国公司 | Method for the synthesis of dialkoxy alkanes by means of the selective oxidation of alcohols |
| CN102105426A (en) * | 2008-07-22 | 2011-06-22 | 阿克马法国公司 | Method for producing dialkoxy alkanes by partial oxidation of lower alcohols in the presence of a catalyst based on molybdenum and iron |
| CN103848727A (en) * | 2012-12-06 | 2014-06-11 | 中国科学院成都有机化学有限公司 | Method of synthesizing dimethoxymethane by methanol catalytic oxidation one-step method |
| DE102013220761A1 (en) * | 2013-10-15 | 2015-04-16 | Robert Bosch Gmbh | Precursor material and method for coating a substrate with a metal chalcogenide layer |
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